Nitrogen → Ethyl 5-amino-2-chloropyrimidine-4-carboxylate

関与物質

反応手順

10% Palladium on carbon (0.2 eq) was added to a N2-flushed mixture of ethyl 2,6-dichloro-5-nitropyrimidine-4-carboxylate (1 eq) and magnesium oxide (2 eq) in 1,4-dioxane (0.15 M). The reaction was purged with H2 under atmospheric pressure at rt. After 16 h additional portions of 10% Pd/C (0.3 eq) and MgO (5 eq) were added and the reaction continued to purge with H2 under atmospheric pressure for 6 h at rt. The crude solids were filtered through a pad of Celite on a paper lined Buchner funnel and washed with CH2Cl2. The filtrate was transferred to a separatory funnel, washed twice with H2O and once with brine, then dried over anhydrous Na2SO4, filtered, and concentrated in vacuo. The crude product was dissolved in CH2Cl2, loaded onto a SiO2 column, and purified by flash chromatography (10-20-30% EtOAc in hexanes) to give ethyl 5-amino-2-chloropyrimidine-4-carboxylate. LC/MS (m/z): 202.0 (MH+).

情報源と証拠